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借助小角X射线光子相关光谱法以及在D2AM光束线上的广角X射线散射研究聚合物动力学的结构依赖性。

Structural dependency of polymer dynamics by means of small-angle X-ray photon correlation spectroscopy and wide-angle X-ray scattering on the D2AM beamline.

作者信息

Stoclet Grégory, Schwaller Duncan, Garlet Romain, Livet Frédéric, Chahine Gilbert A, Blanc Nils, Dupraz Maxime

机构信息

Univ. Lille, CNRS, INRAE, Centrale Lille, Unite Materiaux et Transformations, 59655 Lille, France.

ESRF - The European Synchrotron, 71 Avenue des Martyrs, 38043 Grenoble, France.

出版信息

J Synchrotron Radiat. 2025 May 1;32(Pt 3):649-660. doi: 10.1107/S1600577525001626. Epub 2025 Apr 1.

Abstract

X-ray photon correlation spectroscopy (XPCS) has become a pivotal technique for exploring nanoscale dynamic phenomena across various materials, facilitated by advancements in synchrotron radiation sources and beamline upgrades. The recent Extremely Brilliant Source (EBS) upgrade at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France, has notably improved brilliance and coherence length, thereby enhancing the capabilities of XPCS and related techniques. Here, we present a dedicated setup on the D2AM beamline at the ESRF, enabling simultaneous XPCS and wide-angle X-ray scattering measurements. The setup developed and its performance are detailed in the first part. Then, the XPCS capabilities are evaluated by studying polymer-based materials, with particular attention to the effects of temperature, crystallinity and macromolecular orientation on polymer dynamics. The study on the influence of temperature revealed that XPCS in the case of entangled polymers is an efficient technique to probe the dynamics of the macromolecular network, complementary to classical spectroscopy techniques. In addition, in situ measurements during the polymer crystallization revealed that increased crystallinity slows down macromolecular dynamics. Conversely, studies on stretched samples indicate that macromolecular orientation accelerates these dynamics. This work represents a novel investigation into the effect of crystallinity on macromolecular dynamics using XPCS, opening new avenues for research in polymer science.

摘要

X射线光子相关光谱学(XPCS)已成为探索各种材料纳米级动态现象的关键技术,这得益于同步辐射源的进步和光束线的升级。法国格勒诺布尔欧洲同步辐射装置(ESRF)最近进行的极亮光源(EBS)升级显著提高了亮度和相干长度,从而增强了XPCS及相关技术的能力。在此,我们展示了ESRF的D2AM光束线上的一个专用装置,可实现XPCS和广角X射线散射测量的同时进行。第一部分详细介绍了所开发的装置及其性能。然后,通过研究聚合物基材料评估XPCS的能力,特别关注温度、结晶度和大分子取向对聚合物动力学的影响。对温度影响的研究表明,对于缠结聚合物,XPCS是探测大分子网络动力学的有效技术,可作为经典光谱技术的补充。此外,聚合物结晶过程中的原位测量表明,结晶度增加会减缓大分子动力学。相反,对拉伸样品的研究表明,大分子取向会加速这些动力学。这项工作代表了利用XPCS对结晶度对大分子动力学影响的新研究,为聚合物科学研究开辟了新途径。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6bd4/12067334/a8583cc17008/s-32-00649-fig1.jpg

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